5P82

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 335

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.1
Synchrotron site	BESSY
Beamline	14.1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2014-02-15
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.918409
Spacegroup name	P 1 21 1
Unit cell lengths	45.208, 72.878, 52.504
Unit cell angles	90.00, 109.13, 90.00

Refinement procedure

Resolution	39.369 - 1.220
R-factor	0.1228
Rwork	0.122
R-free	0.13700
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.201
Data reduction software	XDS
Data scaling software	XDS
Phasing software	PHASER (2.5.7)
Refinement software	PHENIX

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	42.710		1.290
High resolution limit [Å]	1.220	3.650	1.220
Rmerge	0.034	0.015	0.330
Rmeas	0.039	0.017	0.384
Total number of observations	353008
Number of reflections	93779	3654	14730
<I/σ(I)>	19.48	74.34	3.47
Completeness [%]	98.2	99.3	95.9
Redundancy	3.764
CC(1/2)	1.000	1.000	0.895

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	4.6	290	0.1 M ammonium acetate, 0.1 M sodium acetate, 24-30% PEG 4000; crystal obtained by streak-seeding and soaked with 90 mM of fragment 335 with the SMILES code COC1=CC=C(Cl)C=C1CN